CN113683892A - Bi-component organic silica gel and preparation method thereof - Google Patents
Bi-component organic silica gel and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention relates to the technical field of silicone rubber, in particular to bi-component organic silicone rubber and a preparation method thereof. The bi-component organic silica gel consists of a component A and a component B, wherein the component A comprises 40-70 parts of modified hydrogen-containing silicone oil A, 20-30 parts of reinforcing resin, 10-25 parts of methyl silicone oil, 15-25 parts of filler and 0.01-0.5 part of catalyst in parts by weight; the component B comprises, by weight, 40-70 parts of modified hydrogen-containing silicone oil B, 20-30 parts of reinforcing resin, 10-25 parts of methyl silicone oil, 15-25 parts of filler and 0.01-1 part of inhibitor. The invention prepares the specific modified hydrogen-containing silicone oil by selecting specific raw materials to prepare the low-viscosity bi-component silica gel with excellent physical properties, no oil production and no hand sticking and ultralow hardness (Shore C zero).
Description
Technical Field
The invention relates to the technical field of silicone rubber, in particular to bi-component organic silicone rubber and a preparation method thereof.
Background
The silicon rubber has excellent cold and heat resistance and durability, is widely applied to daily life of people, such as toothbrushes, amusement equipment, tableware and the like, and the development of the bi-component low-viscosity liquid silicon rubber is gradually advanced along with the improvement of research and development technologies, so that the silicon rubber is widely applied to the industry of adult products because of the advantages of environmental protection, no toxicity, no odor, weather resistance, wide temperature resistance range, small influence of temperature difference on the performance of finished products, skin friendliness, no sensitization, convenient operation, realization of process diversification, extremely wide hardness range and the like.
However, in the process of continuous development of the whole market, the requirement of customers on the experience of products is higher and higher, which puts higher requirements on the performance of raw materials. At present, the low-viscosity liquid silicone rubber on the market generally has the problems of various defects in the performance of the material under ultralow hardness (Shore C zero), for example, the physical properties are poor, the hand feeling is influenced by the hand sticking on the surface, and the subsequent processing of the product, such as oil spraying and packaging, is influenced because the surface oil is not dry.
The invention aims to provide a low-viscosity liquid silicone rubber with excellent physical properties, no oil generation and no hand stickiness and ultra-low hardness (Shore C zero) and a preparation method thereof aiming at the defects of products on the market at present.
Disclosure of Invention
In order to solve the technical problem, the first aspect of the invention provides a bi-component organic silica gel, which consists of a component A and a component B, wherein the raw materials of the component A comprise, by weight, 40-70 parts of modified hydrogen-containing silicone oil A, 20-30 parts of reinforcing resin, 10-25 parts of methyl silicone oil, 15-25 parts of filler and 0.01-0.5 part of catalyst; the component B comprises, by weight, 40-70 parts of modified hydrogen-containing silicone oil B, 20-30 parts of reinforcing resin, 10-25 parts of methyl silicone oil, 15-25 parts of filler and 0.01-1 part of inhibitor.
As a preferable technical scheme of the invention, the raw material of the component A also comprises 0.1-0.16 weight part of coupling agent; the raw material of the component B also comprises 0.1 to 0.16 weight part of coupling agent.
The use of a certain amount of coupling agent in the present invention may enable better presence of the filler in the silicone oil system.
In a preferred embodiment of the present invention, the reinforcing resin is at least one selected from vinyl silicone resin, methyl silicone resin, and phenyl silicone resin.
As a preferable technical scheme of the invention, the number average molecular weight of the methyl silicone resin is 1000-10000.
In a preferred embodiment of the present invention, the filler is at least one selected from silica, silica powder, calcium carbonate, and talc.
As a preferable technical scheme, the modified hydrogen-containing silicone oil A is prepared from raw materials including octamethylcyclotetrasiloxane and tetramethyldisiloxane; the modified hydrogen-containing silicone oil B is prepared from raw materials including octamethylcyclotetrasiloxane, tetramethyldisiloxane and tetramethylcyclotetrasiloxane.
As a preferable technical scheme, the weight ratio of octamethylcyclotetrasiloxane to tetramethyldisiloxane in the raw materials for preparing the modified hydrogen-containing silicone oil A is 300: (30-60).
As a preferable technical scheme of the invention, the weight ratio of octamethylcyclotetrasiloxane, tetramethyldisiloxane and tetramethylcyclotetrasiloxane in the raw materials for preparing the modified hydrogen-containing silicone oil B is 300: (8-12): (50-70).
As a preferable technical scheme of the invention, the hydrogen content of the modified hydrogen-containing silicone oil A is 0.17 wt% -0.3 wt%.
The second aspect of the present invention provides a method for preparing a two-component silicone rubber, comprising the steps of:
(1) preparation of base gum stock a: weighing the raw materials of the component A for later use, dividing the modified hydrogen-containing silicone oil A into 3 parts by weight, respectively marking as A1, A2 and A3, adding A1 and a coupling agent into a kneader, kneading for 5-15 minutes, then adding the filler in portions, kneading for 2-4 hours at room temperature after all the filler is added, heating to 160-170 ℃, and carrying out heat preservation and vacuum banburying for 2-4 hours; then adding A2, and evenly mixing to obtain a basic rubber material A for later use;
(2) preparation of component A: adding the basic rubber material A obtained in the step (1) into A3, reinforcing resin, methyl silicone oil and a catalyst, and uniformly stirring in a planetary stirrer to obtain a component A;
(3) preparation of base rubber compound B: weighing the raw materials of the component B for later use, dividing the modified hydrogen-containing silicone oil B into 3 parts by weight, respectively marking as B1, B2 and B3, adding B1 and a coupling agent into a kneader, kneading for 5-15 minutes, then adding the filler in portions, kneading for 2-4 hours at room temperature after all the filler is added, heating to 160-170 ℃, and carrying out heat preservation and vacuum banburying for 2-4 hours; then adding A2, and evenly mixing to obtain a basic rubber material B for later use;
(4) preparation of the component B: and (2) adding the basic rubber material B obtained in the step (1) into B3, reinforcing resin, methyl silicone oil and an inhibitor, and uniformly stirring in a planetary stirrer to obtain a component B.
As a preferable technical scheme of the invention, the weight ratio of A1, A2 and A3 is (0.8-1.5): (1-2); (3.2-5); the weight ratio of B1 to B2 to B3 is (0.8-1.5): (1-2); (3.2-5).
Has the advantages that:
1. the prepared bi-component silica gel avoids the influence of bubbles in a bi-component silica gel product caused by adding a diluent in a system, and meanwhile, the prepared bi-component silica gel can reach lower viscosity under the condition of not adding the diluent;
2. the low-hardness bi-component silica gel prepared in the system has excellent physical properties under the condition of meeting the requirement of ultralow hardness, and the surface of the low-hardness bi-component silica gel is not sticky and does not produce oil;
3. according to the invention, the specific modified hydrogen-containing silicone oil is prepared by selecting specific raw materials to prepare the low-viscosity bi-component silica gel with excellent physical properties, no oil production and no hand sticking and ultralow hardness (Shore C zero);
4. according to the invention, through the mutual synergistic effect of the specific reinforcing resin and the modified hydrogen-containing silicone oil, the silicon dioxide can be well dispersed in the system and a seamless arrangement structure is formed, so that the oil bleeding phenomenon of the silicone oil is reduced.
Detailed Description
The invention will be further understood by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definition provided in the present disclosure, the definition of the term provided in the present disclosure controls.
As used herein, a feature that does not define a singular or plural form is also intended to include a plural form of the feature unless the context clearly indicates otherwise. It will be further understood that the term "prepared from …," as used herein, is synonymous with "comprising," including, "comprising," "having," "including," and/or "containing," when used in this specification means that the recited composition, step, method, article, or device is present, but does not preclude the presence or addition of one or more other compositions, steps, methods, articles, or devices. Furthermore, the use of "preferred," "preferably," "more preferred," etc., when describing embodiments of the present invention, is meant to refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. In addition, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
In order to solve the technical problem, the first aspect of the invention provides a bi-component organic silica gel, which consists of a component A and a component B, wherein the raw materials of the component A comprise, by weight, 40-70 parts of modified hydrogen-containing silicone oil A, 20-30 parts of reinforcing resin, 10-25 parts of methyl silicone oil, 15-25 parts of filler and 0.01-0.5 part of catalyst; the component B comprises, by weight, 40-70 parts of modified hydrogen-containing silicone oil B, 20-30 parts of reinforcing resin, 10-25 parts of methyl silicone oil, 15-25 parts of filler and 0.01-1 part of inhibitor.
In a preferred embodiment, the raw materials of the component A comprise, by weight, modified hydrogen-containing silicone oil A60-65 parts, reinforcing resin 22-30 parts, methyl silicone oil 15-20 parts, filler 18-22 parts, and catalyst 0.1-0.3 part; the component B comprises 460-65 parts of modified hydrogen-containing silicone oil B, 22-30 parts of reinforcing resin, 15-20 parts of methyl silicone oil, 18-22 parts of filler and 0.1-0.3 part of inhibitor.
In a more preferred embodiment, the raw materials of the component A comprise, by weight, 62 parts of modified hydrogen-containing silicone oil A, 25 parts of reinforcing resin, 18 parts of methyl silicone oil, 20 parts of filler and 0.2 part of catalyst; the component B comprises 62 parts of modified hydrogen-containing silicone oil B, 25 parts of reinforcing resin, 18 parts of methyl silicone oil, 20 parts of filler and 0.2 part of inhibitor.
In one embodiment, the methyl silicone oil is purchased from shin-Etsu or Dow Corning, and the methyl silicone oil in the present invention is shin-Etsu KF96-1000 CS.
In one embodiment, the reinforcing resin is at least one selected from vinyl silicone resin, methyl silicone resin, and phenyl silicone resin, preferably methyl silicone resin.
In one embodiment, the number average molecular weight of the methyl silicone resin is 1000-.
In one embodiment, the filler is selected from at least one of silica, silica powder, calcium carbonate, talc.
In a preferred embodiment, the filler is silica powder.
In order to increase the filling effect, in one embodiment, the average particle size of the silica powder is 500-.
In one embodiment, the silica powder is available from Fujian flying New materials, Inc. under the model YX-900A.
In one embodiment, the methyl silicone resin is available from Jiangxi Xinjiayi New Material Co., Ltd, model number XJY-8205.
In order to increase the mechanical strength of the silicone gel during the preparation of the silicone gel, researchers generally add a certain amount of reinforcing resin into the system, but although the addition of the reinforcing resin increases the strength of the material, the reinforcing resin needs to be cured at high temperature, and the curing time is long, so that the oil bleeding phenomenon occurs. The applicant speculates that the oil bleeding phenomenon of the silicone oil can be reduced because the specific methyl silicone resin in the system has a plurality of methyl branches which are penetrated into the gaps of the modified hydrogen-containing silicone oil to a certain extent, and then the specific silicon dioxide powder is filled in the modified hydrogen-containing silicone oil and the methyl silicone oil to form a seamless arrangement structure.
In one embodiment, the modified hydrogen-containing silicone oil A is prepared from raw materials comprising octamethylcyclotetrasiloxane and tetramethyldisiloxane, wherein the CAS numbers of the raw materials are 556-67-2 and 3277-26-7 respectively.
In one embodiment, the modified hydrogen-containing silicone oil B is prepared from raw materials including octamethylcyclotetrasiloxane, tetramethyldisiloxane and tetramethylcyclotetrasiloxane with CAS numbers of 556-67-2, 3277-26-7 and 2370-88-9 respectively.
In the existing research, in order to increase the tear strength and tensile strength of the silicone rubber, a certain amount of cross-linking agent is often added into the system, but the addition of the cross-linking agent can cause a cross-linking reaction in a vulcanization stage, so that the hardness of the product is relatively high, but if the cross-linking agent is not added, the mechanical strength of the product is slightly reduced, and in order to enable the silicone rubber to have relatively good mechanical strength under the condition of ultralow hardness, the applicant has conducted a great deal of research and finds that the modified hydrogen-containing silicone oil prepared by using octamethylcyclotetrasiloxane, tetramethyldisiloxane or tetramethylcyclotetrasiloxane can achieve the effect. Probably because the polysiloxane chain segment in the modified hydrogen-containing silicone oil prepared can react with components such as methyl silicone oil and methyl silicone resin on one hand to increase the density of a system, and the polysiloxane chain segment in the modified hydrogen-containing silicone oil is more flexible, the molecular chain can be wound and simultaneously drives the distribution of the filler in the system, so that the mechanical strength of the organic silica gel is increased, the modified hydrogen-containing silicone oil also contains the vinyl group of the end group, and the flexible polysiloxane chain segment interacts with the vinyl group and the methyl group in the methyl silicone resin to increase the flexibility of the system, so that the prepared organic silica gel has lower hardness.
In one embodiment, the weight ratio of octamethylcyclotetrasiloxane to tetramethyldisiloxane in the raw materials for preparing modified hydrogen-containing silicone oil a is 300: (30-60), preferably 300: 45.
in one embodiment, the modified hydrogen-containing silicone oil a has a hydrogen content of 0.17 wt% to 0.3 wt%, preferably 0.22 wt%.
In one embodiment, the number average molecular weights of the modified hydrogen-containing silicone oil a and the modified hydrogen-containing silicone oil B are 80000-100000, preferably 90000.
In one embodiment, the weight ratio of octamethylcyclotetrasiloxane, tetramethyldisiloxane and tetramethylcyclotetrasiloxane in the raw materials for preparing modified hydrogen-containing silicone oil B is 300: (8-12): (50-70), preferably 300: 10: 60.
at present, a certain amount of diluent is often added into a system of the organic silica gel with ultralow hardness on the market, but the diluent can cause the generation of bubbles when the organic silica gel is used, and even the problem that the hand feeling is influenced by the hand sticking on the surface is also existed. In the present invention, the applicant has unexpectedly found through extensive studies that a specific hydrogen-containing silicone oil a and a specific hydrogen-containing silicone oil B are prepared by controlling the ratio of raw materials, and thus the ultra-low hardness silicone rubber prepared is not sticky. It is possible that when the ratio of the raw materials is changed, the lengths of the polysiloxane segments of the modified hydrogen-containing silicone oil a and the modified hydrogen-containing silicone oil B are changed, when the polysiloxane segments are too long, the vinyl groups containing the terminal groups are wrapped in the polysiloxane segments, thereby affecting the vulcanization effect, and when the polysiloxane segments are too short, the vulcanization effect of the hydrogen-containing silicone oil a and the hydrogen-containing silicone oil B with other components in the system is reduced.
In one embodiment, the modified hydrogen-containing silicone oil a is prepared by the following steps: adding octamethylcyclotetrasiloxane, tetramethyldisiloxane and a catalyst into a reaction vessel, starting stirring, simultaneously starting heating, reacting at a constant temperature of 60 ℃ for 5 hours, filtering, distilling the filtrate under reduced pressure, and removing low-boiling-point substances to obtain the modified hydrogen-containing silicone oil A.
In one embodiment, the modified hydrogen-containing silicone oil a is prepared with a weight ratio of catalyst to octamethylcyclotetrasiloxane of (30-40): 300, preferably 35: 300.
in one embodiment, the modified hydrogen-containing silicone oil B is prepared by the following steps: adding octamethylcyclotetrasiloxane, tetramethyldisiloxane, tetramethylcyclotetrasiloxane and catalyst into a reaction vessel, starting stirring, simultaneously starting heating, reacting at a constant temperature of 60 ℃ for 5 hours, filtering, distilling the filtrate under reduced pressure, and removing low-boiling-point substances to obtain the modified hydrogen-containing silicone oil B.
In one embodiment, the modified hydrogen-containing silicone oil B is prepared by mixing the catalyst and the octamethylcyclotetrasiloxane in a weight ratio of (30-40): 300, preferably 37: 300.
in one embodiment, the catalyst is selected from one of concentrated sulfuric acid, cation exchange resin, activated clay, potassium hydroxide gel, and potassium trimethylsilanolate, preferably with cation exchange resin.
In one embodiment, the cation exchange resin is available from Rohm and Haas.
According to the invention, the cation exchange resin is selected as the catalyst, so that the prepared modified hydrogen-containing silicone oil has good stability, probably because the cation exchange resin can be directly filtered after preparation, the activity of the modified hydrogen-containing silicone oil cannot be influenced by the residual catalyst, and the cation exchange resin has no corrosivity and peculiar smell, so that the prepared modified hydrogen-containing silicone oil has good performance.
In one embodiment, the raw material of the component A also comprises 0.1 to 0.16 part by weight of a coupling agent, preferably 0.14 part; the raw materials of the component B also comprise 0.1 to 0.16 weight part of coupling agent, preferably 0.14 weight part.
In one embodiment, the coupling agent is a silane coupling agent, and examples of the silane coupling agent include KH-550, KH-570, KH-560, hexamethyldisilazane, hexamethyldisiloxane, and the like, and hexamethyldisilazane is used in the present invention and is available from Nippon silicon chemical Co., Ltd or Jiangxi Lanzhong Sihuo Silicone Co., Ltd.
In one embodiment, the catalyst is a platinum group metal catalyst, such as platinum, rhodium, iridium, palladium or ruthenium series of catalysts, suitable for use in the present system, and platinum series of catalysts, specifically PT-5000 platinum catalyst available from sikon new materials technology ltd, guangzhou, are used in the present invention.
The inhibitor is not limited, and the inhibitor suitable for use in the silicone rubber system is suitable for use in the present invention, and examples of the inhibitor include methylbutynol, ethynylcyclohexanol, polyvinyl polysiloxane, 3, 5-dimethyl-1-hexyn-3-ol, 1-hexyn-1-cyclohexanol, 2-phenyl-3-butyn-2-ol, and the like, and the inhibitor used in the present invention is ethynylcyclohexanol, which is available from Silybum scientific and New materials, Inc., Guangzhou.
In one embodiment, pigments may be added to the A component as needed to obtain different colored silicone gums.
In one embodiment, the weight ratio of the a component to the B component is 1: (0.8-1.5), preferably 1: 1.
the second aspect of the present invention provides a method for preparing a two-component silicone rubber, comprising the steps of:
(1) preparation of base gum stock a: weighing the raw materials of the component A for later use, dividing the modified hydrogen-containing silicone oil A into 3 parts by weight, respectively marking as A1, A2 and A3, adding A1 and a coupling agent into a kneader, kneading for 5-15 minutes, then adding the filler in portions, kneading for 2-4 hours at room temperature after all the filler is added, heating to 160-170 ℃, and carrying out heat preservation and vacuum banburying for 2-4 hours; then adding A2, and evenly mixing to obtain a basic rubber material A for later use;
(2) preparation of component A: adding the basic rubber material A obtained in the step (1) into A3, reinforcing resin, methyl silicone oil and a catalyst, and uniformly stirring in a planetary stirrer to obtain a component A;
(3) preparation of base rubber compound B: weighing the raw materials of the component B for later use, dividing the modified hydrogen-containing silicone oil B into 3 parts by weight, respectively marking as B1, B2 and B3, adding B1 and a coupling agent into a kneader, kneading for 5-15 minutes, then adding the filler in portions, kneading for 2-4 hours at room temperature after all the filler is added, heating to 160-170 ℃, and carrying out heat preservation and vacuum banburying for 2-4 hours; then adding A2, and evenly mixing to obtain a basic rubber material B for later use;
(4) preparation of the component B: and (2) adding the basic rubber material B obtained in the step (1) into B3, reinforcing resin, methyl silicone oil and an inhibitor, and uniformly stirring in a planetary stirrer to obtain a component B.
In one embodiment, the weight ratio of a1, a2, A3 is (0.8-1.5): (1-2); (3.2-5), preferably (1-1.2): (1.3-1.6): (3.8-4.4), more preferably 1: 1.25: 4.1.
in one embodiment, the weight ratio of B1, B2, B3 is (0.8-1.5): (1-2); (3.2-5), preferably (1-1.2): (1.3-1.6): (3.8-4.4), more preferably 1: 1.25: 4.1.
the filling materials added in the steps (1) and (3) can be divided into several times according to the requirements in the preparation process, for example, the filling materials are added in 1 time, 2 times, 3 times and 4 times, the weight of the filling materials added in each time is not limited, the filling materials can be divided into a plurality of parts by weight first, then the filling materials are added in a plurality of parts by weight in sequence, for example, the filling materials are divided into 5 parts by weight at first.
In a third aspect, the invention provides a two-component silicone rubber, and the applications of the two-component silicone rubber comprise adult products (such as silicone rubber dolls), intelligent wearing and robot simulation masks.
As shown in Table 1, the apparatus and the manufacturer used in the present invention.
TABLE 1
Specific examples of the present invention are given below, but the present invention is not limited by the examples.
In addition, the starting materials in the present invention are all commercially available unless otherwise specified.
Examples
Example 1
A bi-component organic silica gel comprises a component A and a component B, wherein the component A comprises 62 parts of modified hydrogen-containing silicone oil A, 25 parts of methyl silicone resin, 18 parts of methyl silicone oil, 20 parts of filler, 0.14 part of coupling agent and 0.2 part of catalyst in parts by weight; the component B comprises raw materials of, by weight, 62 parts of modified hydrogen-containing silicone oil B, 25 parts of methyl silicone resin, 18 parts of methyl silicone oil, 20 parts of filler, 0.14 part of coupling agent and 0.2 part of inhibitor;
the methyl silicone oil is Xinyue KF96-1000 CS;
the number average molecular weight of the methyl silicone resin is 4000;
the filler is silicon dioxide powder; the average particle size of the silicon dioxide powder is 1000 meshes;
the methyl silicone resin is purchased from Xixin exemplary new material Co., Ltd, and has the model of XJY-8205;
the number average molecular weights of the modified hydrogen-containing silicone oil A and the modified hydrogen-containing silicone oil B are 90000;
the hydrogen content of the modified hydrogen-containing silicone oil A is 0.22 wt%; the modified hydrogen-containing silicone oil A is prepared from raw materials of octamethylcyclotetrasiloxane and tetramethyldisiloxane in a weight ratio of 300: 45, a first step of; the preparation method of the modified hydrogen-containing silicone oil A comprises the following steps: adding octamethylcyclotetrasiloxane, tetramethyldisiloxane and a catalyst into a reaction vessel, starting stirring, simultaneously starting heating, reacting at a constant temperature of 60 ℃ for 5 hours, filtering, distilling the filtrate under reduced pressure to remove low-boiling-point substances to obtain modified hydrogen-containing silicone oil A, wherein the weight ratio of the catalyst to the octamethylcyclotetrasiloxane is 35: 300, respectively;
the modified hydrogen-containing silicone oil B is prepared from raw materials of octamethylcyclotetrasiloxane, tetramethyldisiloxane and tetramethylcyclotetrasiloxane in a weight ratio of 300: 10: 60, adding a solvent to the mixture; the preparation method of the modified hydrogen-containing silicone oil B comprises the following steps: adding octamethylcyclotetrasiloxane, tetramethyldisiloxane, tetramethylcyclotetrasiloxane and catalyst into a reaction vessel, starting stirring, simultaneously starting heating, reacting at a constant temperature of 60 ℃ for 5 hours, filtering, distilling the filtrate under reduced pressure to remove low-boiling-point substances to obtain modified hydrogen-containing silicone oil B, wherein the weight ratio of the catalyst to the octamethylcyclotetrasiloxane is 37: 300, respectively;
the catalyst is cation exchange resin; the coupling agent is a silane coupling agent, in particular hexamethyldisilazane; the catalyst is a platinum catalyst; the inhibitor is ethynyl cyclohexanol;
the weight ratio of the component A to the component B is 1: 1;
the preparation method of the bi-component organic silica gel comprises the following steps: (1) preparation of base gum stock a: weighing the raw materials of the component A for later use, dividing the modified hydrogen-containing silicone oil A into 3 parts by weight, respectively recording the parts as A1, A2 and A3, adding A1 and a coupling agent into a kneader, kneading for 12 minutes, then adding fillers in several times, kneading for 3 hours at room temperature after all the fillers are added, heating to 165 ℃, and carrying out heat preservation and vacuum banburying for 3 hours; then adding A2, and evenly mixing to obtain a basic rubber material A for later use; (2) preparation of component A: adding A3, methyl silicone resin, methyl silicone oil and a catalyst into the basic rubber material A obtained in the step (1) and uniformly stirring in a planetary stirrer to obtain a component A; (3) preparation of base rubber compound B: weighing the raw materials of the component B for later use, dividing the modified hydrogen-containing silicone oil B into 3 parts by weight, respectively marking as B1, B2 and B3, adding B1 and a coupling agent into a kneader, kneading for 12 minutes, then adding fillers in portions, kneading for 3 hours at room temperature after all the fillers are added, heating to 165 ℃, and carrying out heat preservation and vacuum banburying for 3 hours; then adding A2, and evenly mixing to obtain a basic rubber material B for later use; (4) preparation of the component B: adding the base rubber material B obtained in the step (1) into B3, methyl silicone resin, methyl silicone oil and an inhibitor, and uniformly stirring in a planetary stirrer to obtain a component B;
the weight ratio of A1 to A2 to A3 is 1: 1.25: 4.1; the weight ratio of B1 to B2 to B3 is 1: 1.25: 4.1; and (3) adding the filler in the step (1) and the step (3) in sequence according to 5 parts by weight.
The silicon dioxide powder is purchased from Fujian flying new materials GmbH and has the model of YX-900A; the cation exchange resin is provided by Rohm and Haas; the hexamethyldisilazane is purchased from new sub-strong silicon chemical corporation; the platinum catalyst is purchased from PT-5000 platinum catalyst of Silicones New Material science and technology Limited, Guangzhou; the ethynylcyclohexanol was obtained from Silicones New materials science and technology, Inc., Guangzhou.
Example 2
A bi-component organic silica gel comprises a component A and a component B, wherein the component A comprises 62 parts of modified hydrogen-containing silicone oil A, 18 parts of methyl silicone oil, 20 parts of filler, 0.14 part of coupling agent and 0.2 part of catalyst in parts by weight; the component B comprises raw materials of, by weight, 62 parts of modified hydrogen-containing silicone oil B, 18 parts of methyl silicone oil, 20 parts of filler, 0.14 part of coupling agent and 0.2 part of inhibitor;
the methyl silicone oil is Xinyue KF96-1000 CS;
the filler is silicon dioxide powder; the average particle size of the silicon dioxide powder is 1000 meshes;
the number average molecular weights of the modified hydrogen-containing silicone oil A and the modified hydrogen-containing silicone oil B are 90000;
the hydrogen content of the modified hydrogen-containing silicone oil A is 0.22 wt%; the modified hydrogen-containing silicone oil A is prepared from raw materials of octamethylcyclotetrasiloxane and tetramethyldisiloxane in a weight ratio of 300: 45, a first step of; the preparation method of the modified hydrogen-containing silicone oil A comprises the following steps: adding octamethylcyclotetrasiloxane, tetramethyldisiloxane and a catalyst into a reaction vessel, starting stirring, simultaneously starting heating, reacting at a constant temperature of 60 ℃ for 5 hours, filtering, distilling the filtrate under reduced pressure to remove low-boiling-point substances to obtain modified hydrogen-containing silicone oil A, wherein the weight ratio of the catalyst to the octamethylcyclotetrasiloxane is 35: 300, respectively;
the modified hydrogen-containing silicone oil B is prepared from raw materials of octamethylcyclotetrasiloxane, tetramethyldisiloxane and tetramethylcyclotetrasiloxane in a weight ratio of 300: 10: 60, adding a solvent to the mixture; the preparation method of the modified hydrogen-containing silicone oil B comprises the following steps: adding octamethylcyclotetrasiloxane, tetramethyldisiloxane, tetramethylcyclotetrasiloxane and catalyst into a reaction vessel, starting stirring, simultaneously starting heating, reacting at a constant temperature of 60 ℃ for 5 hours, filtering, distilling the filtrate under reduced pressure to remove low-boiling-point substances to obtain modified hydrogen-containing silicone oil B, wherein the weight ratio of the catalyst to the octamethylcyclotetrasiloxane is 37: 300, respectively;
the catalyst is cation exchange resin; the coupling agent is a silane coupling agent, in particular hexamethyldisilazane; the catalyst is a platinum catalyst; the inhibitor is ethynyl cyclohexanol;
the weight ratio of the component A to the component B is 1: 1;
the preparation method of the bi-component organic silica gel comprises the following steps: (1) preparation of base gum stock a: weighing the raw materials of the component A for later use, dividing the modified hydrogen-containing silicone oil A into 3 parts by weight, respectively recording the parts as A1, A2 and A3, adding A1 and a coupling agent into a kneader, kneading for 12 minutes, then adding fillers in several times, kneading for 3 hours at room temperature after all the fillers are added, heating to 165 ℃, and carrying out heat preservation and vacuum banburying for 3 hours; then adding A2, and evenly mixing to obtain a basic rubber material A for later use; (2) preparation of component A: adding the basic rubber material A obtained in the step (1) into A3, methyl silicone oil and a catalyst, and uniformly stirring in a planetary stirrer to obtain a component A; (3) preparation of base rubber compound B: weighing the raw materials of the component B for later use, dividing the modified hydrogen-containing silicone oil B into 3 parts by weight, respectively marking as B1, B2 and B3, adding B1 and a coupling agent into a kneader, kneading for 12 minutes, then adding fillers in portions, kneading for 3 hours at room temperature after all the fillers are added, heating to 165 ℃, and carrying out heat preservation and vacuum banburying for 3 hours; then adding A2, and evenly mixing to obtain a basic rubber material B for later use; (4) preparation of the component B: adding the basic rubber material B obtained in the step (1) into B3, methyl silicone oil and an inhibitor, and uniformly stirring in a planetary stirrer to obtain a component B;
the weight ratio of A1 to A2 to A3 is 1: 1.25: 4.1; the weight ratio of B1 to B2 to B3 is 1: 1.25: 4.1; and (3) adding the filler in the step (1) and the step (3) in sequence according to 5 parts by weight.
The silicon dioxide powder is purchased from Fujian flying new materials GmbH and has the model of YX-900A; the cation exchange resin is provided by Rohm and Haas; the hexamethyldisilazane is purchased from new sub-strong silicon chemical corporation; the platinum catalyst is purchased from PT-5000 platinum catalyst of Silicones New Material science and technology Limited, Guangzhou; the ethynylcyclohexanol was obtained from Silicones New materials science and technology, Inc., Guangzhou.
Example 3
A bicomponent silicone rubber, the specific embodiment is the same as example 2, except that a high viscosity vinyl silicone oil having a viscosity of 1000mpa.s is used in place of the modified hydrogen-containing silicone oil a and the modified hydrogen-containing silicone oil B;
the high viscosity vinyl silicon is purchased from Hengji industries organosilicon Co.
Example 4
A bicomponent silicone rubber, the specific embodiment is the same as example 1, except that a high viscosity vinyl silicone oil having a viscosity of 1000mpa.s is used in place of the modified hydrogen-containing silicone oil a and the modified hydrogen-containing silicone oil B;
the high viscosity vinyl silicon is purchased from Hengji industries organosilicon Co.
Example 5
The specific implementation mode of the bicomponent organic silica gel is the same as that in example 1, except that the hydrogen content of the modified hydrogen-containing silicone oil A is 0.5%, and the preparation method of the modified hydrogen-containing silicone oil A comprises the following steps: adding octamethylcyclotetrasiloxane, tetramethyldisiloxane and a catalyst into a reaction vessel, starting stirring, simultaneously starting heating, reacting at a constant temperature of 55 ℃ for 3.8h, filtering, distilling the filtrate under reduced pressure, and removing low-boiling-point substances to obtain the modified hydrogen-containing silicone oil A.
Example 6
The specific implementation mode of the bicomponent organic silica gel is the same as that in example 1, except that the hydrogen content of the modified hydrogen-containing silicone oil A is 0.1%, and the preparation method of the modified hydrogen-containing silicone oil A comprises the following steps: adding octamethylcyclotetrasiloxane, tetramethyldisiloxane and a catalyst into a reaction vessel, starting stirring, simultaneously starting heating, reacting at a constant temperature of 65 ℃ for 6 hours, filtering, distilling the filtrate under reduced pressure, and removing low-boiling-point substances to obtain the modified hydrogen-containing silicone oil A.
Example 7
The specific implementation mode of the bicomponent organic silica gel is the same as that in example 1, except that the commercially available ordinary hydrogen-containing silicone oil without hydrogen-containing double-end-capping end is used for replacing the modified hydrogen-containing silicone oil A and the modified hydrogen-containing silicone oil B;
the commercially available hydrogen-free double-end-enclosure-end-capped common hydrogen-containing silicone oil is purchased from Xinjiayi New Material Co., Ltd, Jiangxi, and has the model of XJY-702B-18.
Performance testing
Preparation of a test piece: a, B components in the examples are respectively mixed, then vacuum defoamed, a certain amount of glue is filled in a cup for curing, a part of glue is molded and formed on a flat vulcanizing machine, and the test piece is prepared.
1. And (3) sticking to hands for testing: the glue materials with fixed amount in the embodiments are respectively taken, cured and formed in a 300ml beaker, placed in an air-conditioned room at 25 ℃ and fully stood, and touched by hands.
2. Oil bleeding test: taking the sizing materials with fixed amount in the embodiment respectively, curing and molding the sizing materials in a 300ml beaker (with the diameter of 70mm), placing the beaker in an air-conditioned room at 25 ℃ for fully standing, paving the rubber blocks on the oil absorption paper, then placing a 500g weight above the rubber blocks, pressing for 24 hours, and testing the diameter of the oil marks on the oil absorption paper.
3. And (3) viscosity testing: the viscosities of the A and B components in the examples were measured separately with a viscometer.
4. And (3) hardness testing: the hardness of the test pieces in the examples was measured with a hardness tester, respectively.
5. And (3) testing mechanical properties: the tensile strength, tear strength and elongation of the test pieces in the examples were measured by a tensile machine.
The test results are shown in Table 2
TABLE 2
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. The bicomponent organic silica gel consists of a component A and a component B, and is characterized in that the raw materials of the component A comprise, by weight, 40-70 parts of modified hydrogen-containing silicone oil A, 20-30 parts of reinforcing resin, 10-25 parts of methyl silicone oil, 15-25 parts of filler and 0.01-0.5 part of catalyst; the component B comprises, by weight, 40-70 parts of modified hydrogen-containing silicone oil B, 20-30 parts of reinforcing resin, 10-25 parts of methyl silicone oil, 15-25 parts of filler and 0.01-1 part of inhibitor.
2. The two-component silicone gum of claim 1, wherein the starting material of component a further comprises 0.1 to 0.16 parts by weight of a coupling agent; the raw material of the component B also comprises 0.1 to 0.16 weight part of coupling agent.
3. The two-component silicone gum of claim 2, wherein the reinforcing resin is at least one selected from the group consisting of vinyl silicone, methyl silicone, and phenyl silicone.
4. The two-component silicone rubber according to claim 3, wherein the methyl silicone resin has a number average molecular weight of 1000-10000.
5. The two-component silicone gum of claim 2, wherein the filler is at least one selected from the group consisting of silica, silica powder, calcium carbonate, and talc.
6. The two-component silicone gum of claim 2, wherein the modified hydrogen-containing silicone oil A is prepared from octamethylcyclotetrasiloxane, tetramethyldisiloxane; the modified hydrogen-containing silicone oil B is prepared from raw materials including octamethylcyclotetrasiloxane, tetramethyldisiloxane and tetramethylcyclotetrasiloxane.
7. The two-component silicone organic gel according to claim 6, wherein the modified hydrogen-containing silicone oil A is prepared from octamethylcyclotetrasiloxane and tetramethyldisiloxane in a weight ratio of 300: (30-60).
8. The two-component silicone organic gel according to claim 6 or 7, wherein the modified hydrogen-containing silicone oil B is prepared from octamethylcyclotetrasiloxane, tetramethyldisiloxane and tetramethylcyclotetrasiloxane in a weight ratio of 300: (8-12): (50-70).
9. The two-component silicone gum of claim 2, wherein the modified hydrogen-containing silicone oil a has a hydrogen content of from 0.17 wt% to 0.3 wt%.
10. A method of preparing a two-component silicone gum as claimed in any one of claims 2 to 9, comprising the steps of:
(1) preparation of base gum stock a: weighing the raw materials of the component A for later use, dividing the modified hydrogen-containing silicone oil A into 3 parts by weight, respectively marking as A1, A2 and A3, adding A1 and a coupling agent into a kneader, kneading for 5-15 minutes, then adding the filler in portions, kneading for 2-4 hours at room temperature after all the filler is added, heating to 160-170 ℃, and carrying out heat preservation and vacuum banburying for 2-4 hours; then adding A2, and evenly mixing to obtain a basic rubber material A for later use;
(2) preparation of component A: adding the basic rubber material A obtained in the step (1) into A3, reinforcing resin, methyl silicone oil and a catalyst, and uniformly stirring in a planetary stirrer to obtain a component A;
(3) preparation of base rubber compound B: weighing the raw materials of the component B for later use, dividing the modified hydrogen-containing silicone oil B into 3 parts by weight, respectively marking as B1, B2 and B3, adding B1 and a coupling agent into a kneader, kneading for 5-15 minutes, then adding the filler in portions, kneading for 2-4 hours at room temperature after all the filler is added, heating to 160-170 ℃, and carrying out heat preservation and vacuum banburying for 2-4 hours; then adding A2, and evenly mixing to obtain a basic rubber material B for later use;
(4) preparation of the component B: and (2) adding the basic rubber material B obtained in the step (1) into B3, reinforcing resin, methyl silicone oil and an inhibitor, and uniformly stirring in a planetary stirrer to obtain a component B.
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